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Method for preparing cyclic carbonate from olefin and carbon dioxide by electrochemical method

A technology of cyclic carbonate and raw material electrochemistry, applied in organic chemistry, electrolytic process, electrolytic components, etc., can solve the problems of large metal material consumption, troublesome separation and purification, and increased cost, and achieve low production cost and excellent reaction system Simple and effective, low material consumption effect

Inactive Publication Date: 2013-01-16
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Chinese patent CN 102127051A has developed a molybdenum acetylacetonate complex / ionic liquid or quaternary ammonium salt catalyst system, using a one-pot intermittent and step-by-step reaction mode to obtain a higher yield of the target product, but there are low efficiency and high energy consumption. Catalysts are more expensive, etc.
The sacrificial anode method not only consumes a large amount of metal materials, increases the cost, but also brings great troubles to the subsequent separation and purification, which is a bottleneck problem hindering the further industrial application of the method

Method used

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  • Method for preparing cyclic carbonate from olefin and carbon dioxide by electrochemical method

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Effect test

Embodiment 1

[0031] With the graphite electrode as the anode and metal nickel as the cathode, add 20mL dimethyl sulfoxide (DMSO for short), 1mmol styrene, 30mmol chlorine in 100mL stainless steel single-chamber high-pressure electrolytic cell lined with polytetrafluoroethylene. Sodium chloride, magnetic stirrer, and carbon dioxide gas to 0.1MPa, sealed; in constant current mode, 0.06A direct current, electrolysis at room temperature for 3 hours, stop power supply; after electrolysis, slowly release unreacted Carbon dioxide gas, the electrolytic solution was distilled under reduced pressure, and then extracted three times with ether, and the target product styrene cyclic carbonate was obtained after the ether volatilized.

[0032] The structure of the resulting product is determined by IR, 1 H NMR, 13 Confirmed by C NMR and GC-MS. The isolated yield of styrene cyclic carbonate was 93%.

Embodiment 2

[0034] With the graphite electrode as the anode and the stainless steel as the cathode, add 20mL of N,N -Dimethylformamide (abbreviation: DMF), 1mmol styrene, 20mmol ammonium chloride, magnetic stirrer, and then introduce carbon dioxide gas to 0.1MPa, seal; in constant current mode, connect 0.06A DC, Electrolyze at room temperature for 3 hours, stop power supply; after electrolysis, slowly release unreacted carbon dioxide gas, distill the electrolyte under reduced pressure, and then extract with ether three times, the target product styrene cyclic carbonate is obtained after the ether volatilizes.

[0035] The structure of the resulting product is determined by IR, 1 H NMR, 13 Confirmed by C NMR and GC-MS. Styrene cyclic carbonate was isolated in 90% yield.

Embodiment 3

[0037]With the graphite electrode as the anode and the brass sheet (i.e. Cu-Sn alloy) as the cathode, add 20mL of DMF, 1mmol of styrene, and 20mmol of bromine to a 100mL stainless steel single-chamber high-pressure electrolytic cell lined with polytetrafluoroethylene. Potassium chloride, magnetic stirrer, and then carbon dioxide gas to 0.1MPa, sealed; in the constant current mode, connected to a 0.06A direct current, electrolyzed at room temperature for 3 hours, stop power; after the electrolysis, slowly let go The reacted carbon dioxide gas, the electrolytic solution was distilled under reduced pressure, and then extracted three times with ether, and the target product styrene cyclic carbonate was obtained after the ether volatilized.

[0038] The structure of the resulting product is determined by IR, 1 H NMR, 13 Confirmed by C NMR and GC-MS. The isolated yield of styrene cyclic carbonate was 92%.

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Abstract

The invention discloses a method for preparing cyclic carbonate from olefin and carbon dioxide by an electrochemical method. By the method, the olefin and the carbon dioxide are used as raw materials, and an inert anode is used for converting the olefin and the carbon dioxide into the cyclic carbonate at a time through an electrochemical reaction at normal temperature and normal pressure in a diaphragm-free single chamber electrolytic tank. According to the method, the olefin and the carbon dioxide which are low in price and readily available are used as the raw materials, so that an oxidant and a catalyst are not required to be added additionally; a sacrificial metal anode is replaced by the inert anode, so that the problem of consumption performance of metal anodes is solved radically; and the method is mild in reaction condition, simple in process operation and low in production cost, has the characteristics of high selectivity, high yield, high efficiency, high economy and environment friendliness, is suitable for appreciation processing of olefin products in petrochemical industries and conversion utilization of the carbon dioxide serving as waste gas generated in petrifaction oil refineries, thermal power plants and other industries, and has economic and environment-friendly benefits.

Description

technical field [0001] The invention belongs to the technical field of electrochemical organic synthesis, and relates to a method for preparing cyclic carbonates, in particular to a method for electrochemically preparing cyclic carbonates using olefins and carbon dioxide as raw materials. . Background technique [0002] Cyclic carbonates are an important class of chemical materials, which can be used as plasticizers, spinning solvents or dispersants for water-soluble dyes and pigments, as well as extractants for olefins and aromatics; they can also be used as raw materials for organic synthesis and precursors for polymer materials; It can also be used as an excellent medium for high-energy batteries and capacitors, and is widely used in organic synthesis, petrochemical, textile and electronic industries. [0003] The traditional synthesis process of cyclic carbonates is based on epoxy compounds and carbon dioxide as raw materials, through homogeneous catalysis or heterogen...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C25B3/02C07D317/36C25B3/23
Inventor 袁高清高晓芳江焕峰
Owner SOUTH CHINA UNIV OF TECH
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